Beruflich Dokumente
Kultur Dokumente
INTRODUCTION
APPARATUS
SETUP
Proper
assembly
of
a
distillation
apparatus
is
essential
in
order
to
ensure
a
successful
distillation.
For
simple
distillations
users
will
use
the
following
equipment:
Distillation
flask
(still):
a
closed
vessel
in
which
the
solution
to
be
distilled
is
heated.
Three-way
adapter:
A
connector
with
three
ports
that
connects
the
distillation
flask
to
the
condenser,
and
also
allows
users
to
insert
a
thermometer
into
the
system.
Condenser:
A
two
chambered
tube
that
cools
product
vapors
using
a
water
jacket.
It
is
very
important
to
have
the
water
inlet
line
attached
to
the
bottom
port
in
order
to
evenly
cool
the
vapor.
Vacuum
adaptor:
A
curved
tube
connecting
the
condenser
to
the
receiving
flask,
which
contains
a
port
to
attach
a
vacuum
if
needed.
Receiving
flask:
A
closed
chamber
that
collects
the
cooled
distillate,
often
accompanied
by
a
ice
bath
to
prevent
re-vaporization
of
highly
volatile
distillate
It
is
also
very
important
when
constructing
the
distillation
apparatus
to
ensure
that
all
connections
are
tightly
sealed.
The
use
of
a
silicon-based
grease
will
help
to
ensure
that
all
connections
are
airtight.
The
loss
of
vapor
from
leaks
will
result
in
low
yields
and
can
cause
contamination
of
the
distillate.
Below
is
a
diagram
depicting
the
correct
setup
of
the
distillation
assembly.
1
James
W.
Zubrick,
The
Organic
Chem
Lab
Survival
Manual,
4th
ED.
(1997)
PROCEDURE
Before
adding
the
solution
to
the
still
it
is
extremely
important
to
determine
which
component
of
the
solution
is
more
volatile
and
note
all
components
boiling
points
to
determine
which
component
will
vaporize
first.
After
the
boiling
points
have
been
determined
the
solution
can
be
added
to
the
distillation
flask
and
heat
can
be
applied.
As
heat
is
added,
the
user
should
closely
monitor
the
vapors
temperature
and
adjust
the
heat
source
to
prevent
drastic
heat
spikes.
Once
the
solution
begins
to
bubble
the
temperature
should
be
held
constant
to
prevent
contamination
of
the
distillate.
It
should
also
be
noted
that
the
solution
will
begin
to
boil
at
an
equilibrium
point
somewhere
between
the
lower
and
higher
boiling
points.
This
is
due
to
the
different
vapor
pressures
of
each
component
and
solutions
vapor
pressure/boiling
point
can
be
determined
using
Raoults
Law:
=
As
the
solution
continues
to
boil
vapor
will
begin
to
move
up
the
three-way
adaptor
and
move
along
the
condenser.
The
condensation
of
the
vapor
is
caused
by
the
drastic
change
in
temperature
caused
by
the
cooling
fluid.
Depending
on
the
component
boiling
points
air
can
be
used
as
the
condensing
fluid,
however
it
is
more
common
to
use
water
due
to
its
higher
specific
heat
capacity,
density,
and
conductivity.
This
allows
water
to
transmit
heat
over
greater
distances
while
using
a
much
lower
volumetric
flow
rate
and
temperature
difference
compared
to
air-cooling.
After
the
fluid
completely
condenses
a
liquid
will
begin
to
drip/flow
into
the
receiving
flask.
As
the
distillate
is
collected
the
user
should
notice
stabilization
of
the
temperature
reading.
During
this
temperature
stabilization
the
most
volatile
component
is
boiling
off
and
the
distillate
collected
is
that
component.
After
all
of
that
component
is
collected
there
should
be
a
spike
in
temperature,
at
this
point
the
collection
flask
should
be
removed
to
prevent
contamination,
and
a
new
one
should
be
connected
if
the
user
is
distilling
a
multicomponent
solution.
Once
all
desired
components
are
collected
the
heat
source
can
be
removed
and
the
apparatus
can
be
disassembled
once
it
has
cooled.
SUMMARY
To
summarize
the
simple
distillation
process,
the
process
begins
when
a
multicomponent
solution
is
charged
into
a
distillation
flask
and
is
heated.
Once
the
solution
begins
to
boil
and
the
temperature
stabilizes.
The
vapor
will
flow
down
the
condenser,
where
it
will
be
cooled
and
be
collected
in
a
receiving
flask.
The
distillate
is
collected
until
the
temperature
begins
to
rise,
at
this
point
distillation
is
stopped
or
a
new
collection
flask
is
added
to
collect
the
next
component.
This
process
is
repeated
until
all
desired
components
are
collected.